CN104419846B - 钛铝锆合金靶材及其制备方法 - Google Patents
钛铝锆合金靶材及其制备方法 Download PDFInfo
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- CN104419846B CN104419846B CN201310412631.XA CN201310412631A CN104419846B CN 104419846 B CN104419846 B CN 104419846B CN 201310412631 A CN201310412631 A CN 201310412631A CN 104419846 B CN104419846 B CN 104419846B
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 37
- 239000000956 alloy Substances 0.000 title claims abstract description 37
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 26
- RTAQQCXQSZGOHL-UHFFFAOYSA-N titanium Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000010936 titanium Substances 0.000 claims abstract description 24
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 24
- 238000007872 degassing Methods 0.000 claims abstract description 20
- 238000003825 pressing Methods 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound 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[Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004411 aluminium Substances 0.000 claims abstract description 16
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- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 12
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[Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Abstract
本发明提供了一种钛铝锆合金靶材及其制备方法。该合金靶材按原子百分比由以下成分组成：钛5‑75%，铝10‑90%，锆1‑20%。其制备方法包括：制备合金粉末、冷等静压处理、脱气处理、热等静压处理以及机加工步骤。本发明的钛铝锆合金靶材具有致密度高、无气孔和偏析，组织均匀，晶粒细小等优点，适用于多种刀具、模具涂层溅射使用。
Description
钛铝锆合金靶材及其制备方法
技术领域
[0001]本发明属于粉末冶金材料及其制备技术领域，特别涉及一种钛铝锆合金靶材及其 制备方法。
背景技术
[0002]自从2〇世纪㈤年代以来，刀具表面涂层技术已经成为提升刀具性能的主要方法。 刀具表面涂层，主要通过提高刀具表面硬度，热稳定性，降低摩擦系数等方法来提升切削速 度，提高进给速度，从而提高切削效率，并大幅提升刀具寿命。
[0003]在金属材料的表面上镀一层TiN、TiCN、TiAl (CN)膜层，来提高工具、模具的耐磨性 能。目前已经开发出纯钛或者钛铝合金靶材来制备这种膜层。研究表明，使用纯钛或钛铝合 金靶材制备的以11'1^1141〇^)等膜层，在工、模具表面可以达到的表面硬度为2400-2800HV，摩擦系数为0.50-0 • 55，最高使用温度为400-60(TC，而在实际应用中，加工不同种 类的材料，对刀具涂层有不同的要求;加工高塑性、高韧性金属材料时，要求刀具涂层自润 滑性能好;现有的氮化钛、氮化钛铝、氮化铬铝等传统涂层，已经无法满足这些使用要求;因 此需要开发多元复合涂层来提高刀具的切削性能，这也对靶材的研发提出了更高的要求； 在众多掺杂的合金元素中，锆由于其独特的结构和优异的性能，倍受青睐。
[0004]目前生产靶材主要有真空熔炼浇铸、热压、热等静压三种工艺。真空熔炼浇铸工艺 生产靶材浇铸过程中容易产生缩孔、疏松和宏观偏析，同时合金中成分与组织的均匀性难 以保证。热压工艺生产靶材生产难以实现大尺寸化，同时热压靶材内部密度分布不均匀，中 部与边缘密度差别可达5%，难以获得高质量高密度的靶材，如公开号为CN102363215A的中 国专利申请所公开的铬铝合金靶材的粉末真空热压烧结制备方法。热等静压法工艺生产靶 材，容易获得均匀细晶结构，靶材密度均匀，能够满足大尺寸靶材的生产，可制得性能优异 的三元合金溅射靶材。
[0005]钛铝锆合金靶材生产技术难度大，因此有关其研宄的文献较少，专利技术更鲜有 之。
发明内容
[0006]针对现有技术的缺陷，本发明的目的在于提供一种钛铝锆合金靶材，该靶材在钛 铝靶材基础上加入元素Zr，可提高所获得涂层的抗磨损性能和使用寿命等。
[0007]本发明的另一目的在于提供一种上述钛铝锆合金靶材的制备方法。该方法可以实 现高品质三元合金钛铝锆合金靶材的制备，而且制备的靶材具有良好的致密性，无气孔、无 疏松和偏析，成分均匀，晶粒细小，规格尺寸大的特点。
[0008]为了实现上述目的，本发明采用了以下技术方案：
[0009] —种钛铝锆合金靶材，按原子百分比由以下成分组成：钛5-75%，铝10-90%，锆1-20%。优选地，上述钛铝锆合金靶材按原子百分比由以下成分组成:钛30%，铝60%，锆10%。 [0010]上述钛铝锆合金靶材的相对密度超过99%，平均晶粒尺寸不大于lOOum。
[0011] 上述钛铝锆合金祀材的制备方法，包括如下步骤：
[0012] 步骤一，合金粉末的制备；
[0013] 步骤二，对制备好的所述合金粉末进行冷等静压处理；
[0014] 步骤三，对所述冷等静压处理后的料坯进行脱气处理；
[0015] 步骤四，对所述脱气处理后的料坯进行热等静压处理；
[0016] 步骤五，对所述热等静压处理后的料坯进行机加工，清洗后得到所需要的成品合 金耙材。
[0017] 在上述制备方法中，所述合金粉末的制备没有特别说明时可以采用本领域常规的 方法，即采用本领域常规方法将原料制成合金粉末。作为一种优选方式，在所述步骤一中， 所述合金粉末的制备可以是采用雾化制粉方法制备合金粉末或者在混料机中直接^将平均 粒径符合要求的原料进行混合来制备合金粉末。当采用混料机进行原料的混合时，更优选 为于真空或惰性气体保护条件下在v型混料机中混合3-5h。
[0018] 在上述制备方法中，作为一种优选方式，在所述步骤一中，所述合金粉末的平均粒 径为30-150wn，不例性地，平均粒径可以为 3〇-50wn、6〇-70iim、120_140um、80-100nni、50wii、 90um、145wn。制备所述合金粉末所用的原料金属钛的纯度优选为99 • 7%以上、金属招的纯度 优选为99.9%以上、金属锆的纯度优选为99 • 9%以上。
[0019] 在上述制备方法中，作为一种优选方式，在所述步骤二中，在20-200MPa压力下进 行冷等静压处理，保压时间为l〇-3〇min。示例性地，所述冷等静压处理时的压力可以为 2 2MPa、30MPa、40MPa、50MPa、65MPa、1 OOMPa、140MPa、155MPa、168MPa、180MPa、190MPa;保压 时间可以为10min、13min、15min、18min、20min。
[0020]在上述制备方法中，作为一种优选方式，在所述步骤三中，所述脱气处理的温度为 300-500°C，脱气时间为5-30h。示例性地，所述温度可以为305°C、320°C、350°C、370°C、400 °C、425°C、450°C、480°C、495°C ;所述脱气时间可以为5h、1 Oh、20h、25h、28h。更优选地，所述 脱气处理时的真空度控制在10 iPa〜10_4Pa，示例性地，真空度可以为10 ipaUO taUO— 3Pa、10-4Pa〇
[0021] 在上述制备方法中，作为一种优选方式，在所述步骤四中，所述热等静压处理的保 温温度为800_130(TC，保温时间为2-5h，压力为120-150MPa。示例性地，所述保温温度可以 为805°C、850°C、920°C、1050°C、1230°C、1296°C ;所述保温时间可以为2h、3h、4.5h、5h;所述 压力可以为123MPa、134MPa、138MPa、145MPa、148MPa、150MPa。
[0022]相比于现有技术而言，本发明具有如下有益效果：
[0023] (1)本发明钛铝锆合金靶材具有致密度高、无气孔和偏析，组织均匀，晶粒细小等 优点。相对密度超过99%，平均晶粒尺寸不大于lOOwn。该靶材适用于多种刀具、模具涂层溅 射使用。采用本发明靶材制备的刀具涂层的自润滑性能好，抗磨损性能和使用寿命均大大 增加。其显微硬度可达到2800〜4500Hv，摩擦系数为0.05〜0.3。
[0024] ⑵本发明方法实现了高品质三元合金钛铝锆靶材的制备。
附图说明
[0025]图1是本发明实施例2得到的靶材的显微组织图。
具体实施方式
[0026]以下通过具体实施例更进一步地描述本发明，但不限于此。
[0027] 实施例1
[0028]本实施例提供的钛铝锆合金靶材由以下原子百分比的成分组成:钛50%，铝40%，锆 10%〇
[0029]本实例钛铝锆靶材的制备方法，包括以下步骤：
[0030]步骤一，按上述靶材成分的设计要求称取纯度为99.6%的金属钛54.6份、纯度为 99 • 7%的金属铝24 • 6份和纯度为99.9%的金属锆20 • 8份，采用雾化制粉工艺制得平均粒径为 40wn的合金粉末（即预合金粉末）；
[0031]所述雾化制粉工艺是采用电弧熔化方法进行金属熔化，并采用惰性气体-金属雾 化制粉方法制备上述合金粉末。
[0032]步骤二，将所得合金粉末装入冷等静压成型模具中，在200MPa的压力下进行冷等 静压处理，保压时间为30min。
[OO33]步骤二，将冷等静压处理后的料述装入尺寸合适的不镑钢包套中，将包套放置在 脱气设备中进行脱气处理，加热温度为50(TC，保温时间为20h，保温时真空度控制在10_2Pa 左右。所述脱气设备可以是市售扩散泵与井式电阻炉。
[0034]步骤四，将脱气完毕的包套封焊后放入热等静压设备中烧结，保温温度为130(TC， 保温时间为5h，压力为120MPa。
[0035]步骤五，对所述热等静压处理后的锭坯进行机加工，清洗后得到所需要的成品合 金革材，其最大尺寸为1040*191*18mm。
[0036] 本实例得到的靶材相对密度达到99%，平均晶粒尺寸1 OOum。
[0037]本实施例得到的靶材经过真空溅射镀在YG8硬质合金刀具表面所制得的涂层，其 显微硬度可达到4000HV，摩擦系数为〇. 2。
[0038] 实施例2 t〇〇39]本实施例提供的钛铝锆合金靶材由以下原子百分比的成分组成，钛9%，铝90%，锆 1%〇
[0040] 本实例钛铝锆靶材的制备方法，包括以下步骤：
[0041] 步骤一，按上述靶材成分的设计要求称取平均粒径为80WI1、纯度为99.6%的钛粉 14 •6份、纯度为的• 7%的铝粉82.3份、纯度为99.5%的锆粉3.1份，将其在V型混料机中混合 3h，混合过程中抽真空进行保护，真空度控制在nr2pa左右；
[0042] 步骤二，将混合好的合金粉末装入冷等静压成型模具中，在150MPa的压力下进行 冷等静压处理，保压时间为1 Omin;
[0043]步骤三，将冷等静压处理后的料坯装入尺寸合适的金属包套中，将包套放置在脱 气设备中进行脱气处理，加热温度350°C，保温时间30h;保温时真空度控制在l(T2Pa左右;所 述脱气设备可以是市售扩散泵与井式电阻炉。
[0044] 步骤四，将脱气完毕的包套封焊后放入热等静压设备中烧结，保温温度为1HKTC， 保温时间3h，压力150MPa;
[0045]步骤五，对所述热等静压处理后的锭坯进行机加工，清洗后得到所需要的成品合 金靶材，其尺寸为741*191*18mm。
[0046] 本实例得到的靶材相对密度达到99.2%，平均晶粒尺寸70wn，从图1中可以看出，本 实施例得到的靶材致密度高、无气孔和偏析，组织均匀，晶粒细小。
[0047] 本实施例得到的靶材经过真空溅射镀在YG8硬质合金刀具表面制得的涂层，其显 微硬度可达到2800Hv，摩擦系数为0 • 3。
[0048] 实施例3
[0049] 本实施例提供的钛铝锆合金靶材由以下原子百分比的成分组成，钛5%，铝75%，锆 20% 〇
[0050] 本实例钛铝锆靶材的制备方法，包括以下步骤：
[0051] 步骤一，按上述靶材成分的设计要求称取平均粒径为150wn、纯度为99 • 6%的钛粉 5.9份、纯度为99 • 7%的铝粉49.5份、纯度为99 • 5%的锆粉44.6份，将其在V型混料机中混合 5h，混合过程中充入高纯氩气进行保护；
[0052]步骤二，将混合好的粉末装入冷等静压成型模具中进行冷等静压处理，冷等静压 压力为200MPa，保压时间为20min;
[0053]步骤三，将冷等静压料坯装入尺寸合适的金属包套中，将包套放置在脱气设备中 进行脱气处理，加热温度为300°C，保温时间为15h;保温时真空度控制在10 3Pa左右;所述脱 气设备可以是市售扩散泵与井式电阻炉。；
[0054]步骤四，将脱气完毕的包套封焊后放入热等静压设备中烧结，保温温度为125(TC， 保温时间4h，压力135MPa;
[0055]步骤五，对所述热等静压处理后的锭坯进行机加工，清洗后得到所需要的成品合 金革巴材，其尺寸为800*191*18_。
[0056] 本实例得到的靶材相对密度达到"• 7%，平均晶粒尺寸90_。
[0057]本实施例得到的靶材经过真空溅射镀在YG8硬质合金刀具表面所制得的涂层，其 显微硬度可达到3000Hv，摩擦系数为0.05。
[0058] 实施例4
[0059]该实施例提供的钛铝锆合金靶材由以下原子百分比的成分组成，钛75%，铝10%，锆 15%〇
[0060] 本实例钛铝锆靶材的制备方法，包括以下步骤：
[0061] 步骤一，按上述靶材成分的设计要求称取平均粒径为30WH、纯度为99.6%的钛粉 68.7份、纯度为99_7%的铝粉5_2份、纯度为99.5%的锆粉26.1份，将其在V型混料机中混合 4h，混合过程中充入高纯氩气进行保护；
[0062]步骤二，将混合好的粉末装入冷等静压成型模具中进行冷等静压处理，冷等静压 压力为20MPa，保压时间为30min;
[0063]步骤三，将冷等静压料坯装入尺寸合适的不锈钢包套中，将包套放置在脱气设备 中进行脱气处理，加热温度为40(TC，保温时间为5h;保温时真空度控制在l〇_4Pa左右，所述 脱气设备可以是市售扩散泵与井式电阻炉。；
[00M]步骤四，将脱气完毕的包套封焊后放入热等静压设备中烧结，保温温度为8〇(TC， 保温时间为2h，压力为140MPa;
[0065]步骤五，对所述热等静压处理后的锭坯进行机加工，清洗后得到所需要的成品合 金革El材，其尺寸为1000*200* 18mm。
[0066] 本实例得到的靶材相对密度达到99 • 7%，平均晶粒尺寸80mi。
[0067]本实施例得到的靶材经过真空鹏射镀在YG8硬质合金刀具表面所制得的涂层，其 显微硬度可达到4500HV，摩擦系数为0.08。
[0068] 实施例5
[0069]本实施例提供的钛铝锆合金靶材由以下原子百分比的成分组成，钛30%，铝60%，锆 10%。
[0070] 该靶材的制备方法同实施例2，得到的粑材尺寸为1100*180*23mm。
[0071] 本实例得到的靶材相对密度达到99.8%，平均晶粒尺寸65um。
[OO72]使用该成分靶材经过真空漉射镀在YG8硬质合金刀具表面制得涂层，其显微硬度 可达到4450Hv，摩擦系数为0.09。
[0073]以上实施例中各参数的测定方法如下：相对密度采用阿基米德排水法进行测定； 通过光学金相显微镜对靶材晶粒尺寸进行分析;用显微维式硬度计对刀具涂层显微硬度进 行检测;采用STF-A摩擦系数仪对刀具涂层摩擦系数进行测定。
[0074]应当理解，这些实施例的用途仅用于说明本发明而非意欲限制本发明的保护范 围。此外，也应理解，在阅读了本发明的技术内容之后，本领域技术人员可以对本发明作各 种改动、修改和/或变型，所有的这些等价形式同样落于本申请所附权利要求书所限定的保 护范围之内。
Claims (1)
1. 一种钛铝锆合金靶材，其特征在于，该靶材按原子百分比由以下成分组成:钛:75%， 铝:10%，锆:15% ;所述靶材的制备方法包括如下步骤： 步骤一，按所述靶材成分组成要求称取平均粒径为30wn、纯度为⑽• 6 %的钛粉6S • 7份、 纯度为99 • 7 %的铝粉5 • 2份和纯度为99.5 %的锆粉26.1份，在V型混料机中混合4h，混合过 程中充入高纯氩气进行保护； 步骤二，将混合好的粉末装入冷等静压成型模具中进行冷等静压处理，所述冷等静压 的压力为20MPa，保压时间为30min; 步骤三，将冷等静压料坯装入尺寸合适的不锈钢包套中，将包套放置在脱气设备中进 行脱气处理，加热温度为400°C，保温时间为5h;保温时真空度控制在4Pa左右，所述脱气 设备是市售扩散泵； 步骤四，将脱气完毕的包套封焊后放入热等静压设备中烧结，保温温度为800°C，保温 时间为2h，压力为140MPa; 步骤五，对所述热等静压处理后的锭坯进行机加工，清洗后得到所需要的成品合金靶 材，尺寸为 1000*200*18mm。
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